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目的研究高效液相色谱-质谱联用法(HPLC-MS/MS)测定血浆中二亚油酰磷脂酰胆碱(DLPC)浓度测定的方法。方法 2010年11月-2011年1月,7例受试者,3例服用多烯磷脂酰胆碱软胶囊(试验制剂),3例服用多烯磷脂酰胆碱胶囊(参比制剂),1例未服药;采集服药者血浆,对各种检测方法、样品预处理条件进行考核;用建立的方法对6例服药者和1例未服药者血浆DLPC浓度进行测定。结果最终建立的方法为:采用API 3000型HPLC-MS/MS液质联用系统,多反应离子检测模式,正离子扫描,大气压化学电离源,色谱柱为Ultimate CN分析柱(50.0 mm×4.6 mm,5μm),流动相为甲醇︰水︰甲酸(80︰20︰0.05,V/V/V),流速为0.5 mL/min,格列齐特作为内标。受试者口服多烯磷脂酰胆碱软胶囊试验制剂与参比制剂后,DLPC血浆浓度水平均未见明显的变化规律。未服药者血浆DLPC浓度也有较高浓度水平。结论所建立的HPLC-MS/MS法,未能用于多烯磷脂酰胆碱软胶囊生物等效性评价。
Objective To study the method for the determination of diltiazem phosphatidylcholine (DLPC) in plasma by high performance liquid chromatography-mass spectrometry (HPLC-MS / MS). Methods From November 2010 to January 2011, 7 subjects, 3 polyene phosphatidylcholine soft capsules (test preparation), 3 polyene phosphatidylcholine capsules (reference preparation), 1 The patients were taken without medication. Blood samples were taken from the plasma of the drug-eluting patients to evaluate the detection methods and sample pretreatment conditions. The plasma concentrations of DLPC in 6 patients and 1 patient were measured by the established method. The final results were as follows: The API 3000 HPLC-MS / MS LC / MS system, multiple reaction mode, positive ion scan and atmospheric pressure chemical ionization were used. The column was an Ultimate CN column (50.0 mm × 4.6 mm , 5μm). The mobile phase consisted of methanol: water: formic acid (80:20:0.05, V / V / V) at a flow rate of 0.5 mL / min and gliclazide as internal standard. Subjects oral polyene phosphatidylcholine soft capsule test preparation and reference preparation, DLPC plasma concentration levels showed no significant change. Plasma concentrations of DLPC did not take a higher concentration levels. Conclusion The established HPLC-MS / MS method failed to evaluate the bioequivalence of polyene phosphatidylcholine soft capsules.